slocum



FRANK LSLOCUM, OF PITTSBURGH, PENN$Y LVANIA, ASS-IGNDR T0 JAMES HENRY REID, OF PITTSBURGH, I fENNSYLVAIHA.

PRQCESS F011. THE FIXATION 01" NTETAJG-EN,

No Drawing.

To all whom it may concern:

Be it known that I, FRANK L. Snoomu, a citizen of the United States, and resident of Pittsburgh, in the county of Allegheny and State of Pennsylvania, have invented a new and useful Improvement in Processes for the Fixationof Nitrogen; and I do hereby declare the following to bee full, clear, and exact description thereof.

My invention relates to the process of efiecting a combination between nitrogen gas and a carbid whereby nitrogen-contain.- ing products are secured at lower temperatures and in shorter time than has been possible heretofore.

This application is filed as a continuation in part of my application, Serial No. 190,-

.565, filed September 10, 1917.

I produce the acceleration of the reaction and the lowering of the necessary temperature by means of catalytic agents which may be used separately or combined in any ratio that may appear. desirable. One "class of catalysts consists ,of carbon-haloid compounds, such as carbon tetrachlorid, for example.

The carbid can be as such or mixed with a suitable amount (1 to 5%, for example) of alkaline salt-such as sodium carbonate-0r alkaline hydratesor oxids, or other compounds having great affinity for chlorin.

The second class of catalysts consists of the product resulting from the action of nitrogen upon a'carbid. This nitrogen-can bon is an active auto-catalyst. For the purpose here described it is immaterial Whether this catalyst be formed in the presence of any other catalyst, or whether the material used be fully saturated with nitrogen or not, as I have discovered that the admixture with a carbid of a nitrogen-containing material resulting from the action of nitrogen on a carbid and the subsequent exposure of the mixture to the action of nitrogen gas at a suitable temperature results in the absorption of nitrogen at a lower temperature and in less'time than is the case when carbid alone is exposed to the action of nitrogen.

In describing a particular nrethod of procedure for carrying out my process, it is understood that I may vary the steps of the method both in order and arrangement within the scope of the appended claims.

The method which I prefer to use for ac- I Specification of Letters Patent.

Patented (Pet. 1%, iifiil Application filed November 27, 1917. Serial No. 264,184.

'celerating the reaction by means of a carbon-haloid compound, such as carbon tetrachlorid, is as follows: A commercial car-- terial.

\Vhen the conditions as stated above are carried out, the absorption of nitrogen takes place in about three hours, and the heat of the reaction is not as great as when the reaction takes its normal course and, there fore, the temperature of the mass does not reach a point where cyanids are formed. This is-a valuable feature of the process, as the presence of cyanide in the final product is a decided disadvantage, since the production of ammonia is made more ditiicnlt, and

if it is intended to use the product as fertilizer the presence of cyanids (which are deadly poisons) may result in much injury.

A further advantage of the use of the particular catalyst here described that, being perfectly mixed with the gas and being itself a gas under furnace conditions, it

-thoroughly difi'used throughout the system and acts in amore eflicie nt manner than can be the case with a solid catalyst.

A solid catalyst can only act at its own surface, which is very small in comparison with the total surface of the carbid particles, unless so much of the solid catalyst be used as to result in the presence of a large amount of inert matter in the product. i

The nitrogen-containing material resulting from the interaction of a carbid with nitrogen may be used as a catalyst as follows, though it is to understood that I do not limit myself to the exact method of procedure or amount of catalyst here stated.

A carbid, as calcium carbid, for example, is crushed to about forty-mesh size and mixed with from 2 to 5% by weight of the powdered nitrogen-containing product obtained by acting on a carbidwith nitrogen a DJ gas at atemperature such that nitrogen is absorbed by and enters into combination hours and an atmosp with nitrogen and is practically free of cywith the metal of the carbid. This mixture is introduced into a suitably designed retort and the retort is maintained at about 750 Cent. during a eriod of four to six liere of nitrogen gas maintained within said retort. The temperature of the mass is kept below l000 Cent, and the resulting product is saturated anids.

Whenever it is desirable, the two cata-.

lysts described above may be used in conjunction by exposing the mixture of carbid and nitrified material to nitrogen gas containing a carbon-haloid compound while maintaining the retort at a temperature of approximately 750 Cent. By using this mixture, it is possible to get the greater acceleration due to a gas catalyst without the necessity of introducing more than 1 to 2% by volume of the gas catalyst into the nitrogen. I

The use of the nitrogen-containing material as a catalyst has a very great advantage over all other solid catalysts, in that no inert material is left in the product as,- taken from the furnace, since the nitrogen in the catalytic material is not lost bythe reaction.

While I have indicated certain particular materials or compounds of materials which may be used in carrying out the invention, and also have described the various steps of the processes which may be carried out, it

.is to be understood that the invention is not gen which consists in mixing a carbid witha compound formed by reaction between a carbid and nitrogen as a catalyst, and treating the same, with nitrogen in the presence of a carbon-haloid compound.

3. The process for the fixation of nitrogen which consists in 'introducing a carbonhaloid-vapor and nitrogen gas into a car bid, and maintaining the carbid at a temperature necessary to cause-the required fixation. Y

4. The process for. the fixation 'of nitrogen which consists in introducing carbon-' tetrachloridin gaseous formalong with' nitrogen gas into a carbid while maintaining the latter at'atemperaturefor accomplishing the fixation of the nitrogen.

' 5. The process for the fixation of nitrogen which consists in introducing carbontetrachlorid in gaseous form along with nitrogen gas into a carbid while maintaining the same excluded from the air and at a tem perature for accomplishing the fixation of the nitrogen.

6.'The process for'the fixationof nitrogenwhich consists in mixing a carbid with an alkaline salt, introducing a carbon-haloid vapor'and nitrogen together into such carbid and salt and maintaining the mixture .at a temperature to accomplish the fixation of the nitrogen. I

7. The process for the fixation of nitrogen which consists in mixing a carbid and a completely nitrified materlal, introducing nitrogen gas, and maintaining the compound at a temperature for the-fixationof the nitrogen. 8. The process for the fixation of nitrogen which consists in treating a carbid with carbon-tetrachlorid, and introducing nitrogen gas while maintaining the compound at a temperature to cause the fixation of the.

nitrogen.

9. The process for the fixation of nitrogen which consists in mixing a carbid with an alkaline salt, treating the mixture with carbon-tetrachlorid, and introducing nitrogen gas to the mixture while maintaining the said mixture at a temperature to cause the fixation of the nitrogen.

In testimony whereof I, the said FRANK L. SLocUM, have hereunto set my hand.

FRANK L. SLOOUM. Witnesses:

' J. M. DEVANEY, W. J. BOLAND.

Certificate of Correction.

It is hereby certified that Letters Patent No. 1,318,929, granted October 14,

1919, upon the application of Frank L. Slocum of Pittsburgh, Pennsylvania, for an improvement in Processes for the Fixation of Nitrogenf were erroneously issued to James Henry Reid, of Pittsburgh, Pennsylvania, whereas said Letters Patent should have been issued to International i Vtrogen- Com-puny, a 007"?)07Th z'on of Dela-ware, said corporation being assignee, by mesne assignments, of the entire interest in said invention as shown by the records of assignments in this oifice; and that the said Letters Patent should be read with this correction therein that the same may conform to the record 01 the case in the Patent Office.

Signed and sealed this 17th day of April, A. 1). 1922 SEAL KARL FENNING,

Acid 22g Commissioner 0/ Patents. 

